Engineering topics
Volz, M.
Publications and source records attributed to Volz, M..
Bridgman Growth of Germanium and Germanium-Silicon Crystals under Microgravity
Four different Bridgman growth experiments on Ge:Ga and Ge(sub x)Si(sub 1-x) were performed under microgravity during the FOTON M4 flight in fall 2014 as joint German-Russian experiments. The experiments were also part of the RDGS/ICESAGE project(s) of ESA/NASA on detached growth of Ge and Ge-Si. Three experiments on Ge:Ga investigated different heat and mass transport regimes, i.e. mostly diffusive conditions, flows driven by a rotating magnetic field, and flows driven by vibration. The fourth experiment on Ge(sub 0.98)Si(0.02) investigated detached growth. All four experiments were successful and yielded crystals. Both the Ge-Si experiment and two of the Ge:Ga experiments showed stable detachment from the ampoule wall, although this was not planned for the latter two experiments. The influence of the rotating magnetic field as well as of the vibration was pronounced in the case of the microgram experiments, but dominated by buoyancy convection under 1g.
Bridgman Growth of Germanium and Germanium-Silicon Crystals Under Microgravity
No abstract available
Initial Transient in Zn-doped InSb Grown in Microgravity
Three Zn-doped InSb crystals were directionally solidified under microgravity conditions at the International Space Station (ISS) Alpha. The distribution of the Zn was measured using SIMS. A short diffusion-controlled transient, typical for systems with k greater than 1 was demonstrated. Static pressure of approximately 4000 N/m2 was imposed on the melt, to prevent bubble formation and dewetting. Still, partial de-wetting has occurred in one experiment, and apparently has disturbed the diffusive transport of Zn in the melt.
Dewetting and Segregation of Zn-Doped InSb in Microgravity Experiments
In directional solidification, dewetting is characterized by the lack of contact between the crystal and the crucible walls, due to the existence of a liquid meniscus at the level of the solid-liquid interface. This creates a gap of a few tens of micrometers between the crystal and the crucible. One of the immediate consequences of this phenomenon is the dramatic improvement of the quality of the crystal. This improvement is partly due to the modification of the solid-liquid interface curvature and partly to the absence of sticking and spurious nucleation at the crystal-crucible interface. Dewetting has been, commonly observed during the growth of semiconductors in crucibles under microgravity conditions where it appears to be very stable: the gap between the crystal and the crucible remains constant along several centimetres of growth. The physical models of the phenomenon are well established and they predict that dewetting should not occur in microgravity, if sufficient static pressure is imposed on the melt, pushing it towards the crucible. We present the results of InSb(Zn) solidification experiments conducted at the International Space Station (ISS) where, in spite of a spring exerting a pressure on the liquid, partial dewetting did occur. This surprising result is discussed in terms of force exerted .by the spring on the liquid and of possibility that the spring did not work properly. Furthermore, it appears that the segregation of the Zn was not affected by the occurrence of the dewetting. The data suggest that there was no significant interference of convection with segregation of Zn in InSb.
Te-and Zn-Doped InSb Crystals Grown in Microgravity
In 2002, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation, seven doped InSb crystals were grown in microgravity at the International Space Station. The key goals of the SUBSA investigation are: (a) to clarify the origin of the melt convection in space laboratories; (b) to reduce melt convection to the level which allows reproducible diffusion-controlled segregation; (e) to explore the submerged baffle process and liquid encapsulation in microgravity. 30 crystal growth experiments were conducted in the ground unit, to optimize the design of flight ampoules and to test the transparent SUBSA furnace developed by TecMasters Inc. The specially designed furnace, allowed observation of the crystal growth process (melting, seeding, motion of the solid-liquid interface, etc.). In the summer of 2002, eight crystal growth experiments were conducted in the Microgravity Science Glovebox (MSG) facility at the ISS. Four Te-doped (k = 0.5) and three Zn-doped (k2.9) crystals were grown on undoped seeds. In one experiment, we were not able to seed and grow. The seven grown crystals were sectioned and analyzed using SIMS. The design of the SUBSA ampoules, the segregation data and the video images obtained during the SUBSA flight experiments will be presented and discussed.
Detached Growth of Germanium by Directional Solidification
Detached crystal growth technique (dewetting) offers improvement in the quality of the grown crystals by preventing sticking to the walls of the crucible and thus reducing the possibility of parasitic nucleation and formation of lattice defects upon cooling. One of the factors relevant for the phenomena is the pressure differential across the meniscus at the crystal-melt interface. We investigated this effect experimentally. The growth took place in closed ampoules under the pressure of an inert gas (forming gas: 96% Ar + 4% H2). The pressure above the melt was adjustable and allowed for a control of the pressure difference between the top and bottom menisci. The crystals were characterized, particularly by taking profilometer measurements along the grown crystals surface. The effects of the experimental conditions on the detachment were compared with those predicted based on the theory of Duffar et al.
Solidification Using a Baffle in Sealed Ampoules (SUBSA)
Solidification Using a Baffle in Sealed Ampoules (SUBSA) will be the first materials science experiment conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. The launch is schedule for May 31, 2002. Using the specially developed furnace, 10 Te and Zn-doped single crystals of InSb will be directionally solidified in microgravity. A key goal of the SUBSA investigation is to (i) clarify the origin of the melt motion in space laboratories and (ii) to reduce the magnitude of the melt motion to the point that it does not interfere with the transport phenomena. These goals will be accomplished through a special ampoule and furnace design. A disk-shaped baffle, positioned close to the freezing front, is used to reduce melt motion. Furthermore, the solidification will be visualized by using a transparent furnace, with a video camera, continuously sending images to the earth. This allows detection of bubbles and melt de-wetting that could cause surface tension driven convection. In preparation for the space experiments, 30 ground-based experiments were conducted. The results of ground based tests and numerical modeling will be presented. Based on numerical modeling, 12 mm 1D silica ampoules were selected. The small diameter ampoule favors closer placement of the baffle to the interface, without excessive radial segregation caused by forced convection while providing more damping of natural convection. The parts in the silica ampoule include 2 carbon springs made by Energy Science Laboratories, Inc., a pyrocarbon-coated graphite cylinder, pyrocarbon-coated graphite a baffle with the shaft and the InSb charge with the seed crystal grown by W.A. Bonner of Crystallod Inc.
Space- and Ground-Based Crystal Growth Using a Baffle (CGB)
The composition of semiconductor crystals produced in space by conventional melt-growth processes (directional solidification and zone melting) is affected by minute levels of residual micro-acceleration, which causes natural convection. The residual acceleration has random magnitude, direction and frequency. Therefore, the velocity field in the melt is apriori unpredictable. As a result, the composition of the crystals grown in space can not be predicted and reproduced. The method for directional solidification with a submerged heater or a baffle was developed under NASA sponsorship. The disk-shaped baffle acts as a partition, creating a small melt zone at the solid-liquid interface. As a result, in ground based experiment the level of buoyancy-driven convection at the interface is significantly reduced. In several experiments with Te-doped GaSb, nearly diffusion controlled segregation was achieved.
Contact Angles and Surface Tension of Germanium-Silicon Melts
Precise knowledge of material parameters is more and more important for improving crystal growth processes. Two important parameters are the contact (wetting) angle and the surface tension, determining meniscus shapes and surface-tension driven flows in a variety of methods (Czochralski, EFG, floating-zone, detached Bridgman growth). The sessile drop technique allows the measurement of both parameters simultaneously and has been used to measure the contact angles and the surface tension of Ge(1-x)Si(x) (0 less than or equal to x less than or equal to 1.3) alloys on various substrate materials. Fused quartz, Sapphire, glassy carbon, graphite, SiC, carbon-based aerogel, pyrolytic boron nitride (pBN), AIN, Si3N4, and polycrystalline CVD diamond were used as substrate materials. In addition, the effect of different cleaning procedures and surface treatments on the wetting behavior were investigated. Measurements were performed both under dynamic vacuum and gas atmospheres (argon or forming gas), with temperatures up to 1100 C. In some experiments, the sample was processed for longer times, up to a week, to investigate any changes of the contact angle and/or surface tension due to slow reactions with the substrate. For pure Ge, stable contact angles were found for carbon-based substrates and for pBN, for Ge(1-x)Si(x) only for pBN. The highest wetting angles were found for pBN substrates with angles around 170deg. For the surface tension of Ge, the most reliable values resulted in gamma(T) = (591- 0.077 (T-T(sub m)) 10(exp -3)N/m. The temperature dependence of the surface tension showed similar values for Ge(1-x)Si(x), around -0.08 x 10(exp -3)N/m K, and a compositional dependence of 2.2 x 10(exp -3)N/m at%Si.
Detached and Floating-Zone Growth of Semiconductor Crystals on the ISS
Understanding the mechanism of detached Bridgman growth and establishing the growth of large scale germanium-silicon crystals by the float-zone technique are the key points of the project "RDGS - Reduction of Defects in Germanium-Silicon". The contact angle of the melt and the growth angle of the crystal are essential parameters which allow a controlled use of detached growth. The contact angle was determined for a variety of different substrates and melt compositions; pBN showed the highest value for pure germanium as well as for germanium-rich GeSi melts. The growth angle of Ge(sub 0.95) Si(sub 0.05) was measured to be 8.5-10.5 degrees which concurs with the values of pure germanium and silicon, respectively. The temperature dependence and the concentration dependence of the surface tension were determined for concentrations up to 10at% silicon (partial derivative (gamma)/partial derivative T=-0.08 (raised dot) 10(exp -3)N/m (raised dot) K, partial derivative (gamma)/partial derivative (C)=2.2 (raised dot) 10(exp -3)N/m (raised dot) at%). Using these values, the critical Marangoni number indicating the transition to time-dependent thermocapillary flow will be exceeded for the growth of large scale float-zone crystals onboard the ISS. Therefore, suitable tools for flow control are required.
Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors
The objective of this research is to investigate the influences of gravitationally-dependent phenomena (hydrostatic and buoyant) on the growth and quality of doped and alloyed Cadmium-Zinc-Telluride (CdZnTe) crystals grown by the modified seeded Bridgman-Stockbarger technique. It is hypothesized that the damping of the gravitationally-dependent buoyancy convection will substantially enhance chemical homogeneity and the near-elimination of hydrostatic pressure will enable significant reduction in defect (dislocations and twins) density.
Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport
Complete and systematic ground-based experimental and theoretical analyses on the Physical Vapor Transport (PVT) of ZnSe and related ternary compound semiconductors have been performed. The analyses included thermodynamics, mass flux, heat treatment of starting material, crystal growth, partial pressure measurements, optical interferometry, chemical analyses, photoluminescence, microscopy, x-ray diffraction and topography as well as theoretical, analytical and numerical analyses. The experimental results showed the influence of gravity orientation on the characteristics of: (1) the morphology of the as-grown crystals as well as the as-grown surface morphology of ZnSe and Cr doped ZnSe crystals; (2) the distribution of impurities and defects in ZnSe grown crystals; and (3) the axial segregation in ZnSeTe grown crystals.